Process of producing bitumenlike materials from coal



May 18, 1943 A. JENKNER PROCESS OF PRODUCING BITUMEN-LIKE MATERIALS FROMGOAL 2 Sheets-Sheet 1 ROM Filed Oct. 15, 1940 m i a.. R mm m f v km w a4 T @Mw l ms H l A i llr .I .L. W/ J -QN b I|;T\ J/ I I :1 .%N L N wmw/.m

May 18, 1943 A. JENKNER PROCESS OF "PRODUCING BITUMEN-LIKE MATERIALSFROM COAL Filed Oct. 15, 1940 2 Sheets-Sheet 2 mema'ms s, 194a UNITED,STATES PATENT opt-1 3 rnocass' F rnonuomo BITUMENLIKE MATERIALS momcoax.

Application 0ctober15, 1940, Serial No. 361,317 In Germany October 6,1939 12 Claims. (Cl.196 14) The invention relates to the production from7 coal or bitumen-like materials, 1. e., substances of a' colloidalcharacter similar. to that of the mineral oil bitumen.

According to the invention the coal in pulveru lent condition isheat-treated with solventsnamely, hydrocarbon oils having a high boilingpoint; then part of the solvent isdistilled without separation of theundissolved proportions.

The result is a bitumen-like residue which may be used for varyingpurposes, particularly as a substitute for bitumen used heretofore forthe insulation of pipes,

It is known to extract coal with hydrocarbon oils having a high boilingpoint, to separate the undissolved matter after the extraction and todistill solvents, if necessary. In this manner it was possible toproduce pitch-like materials which, however, differ materially from theproduct made in accordance with the invention.

It was also known to heat coal with tar to comparatively hightemperatures, namely to such temperatures where a-dccomposition of thecoal occurs, and then to use the .obtained product without separatingthe solid substances. Also this known process results in products whichdiifer from those made in accordance with the invention, in thesamemanner as the processes for making fluent coal where coal with oils isworked into a stable suspension.

With all of these known processes, the production of bitumen-likesubstances was neither a intended nor achieved. s

In solving this problem, a number of process conditions must be observedto obtain the result desired. I

Thus it has been-found that a bitumen-like product cannot be made fromevery mineral coal, but that it is necessary to use glance coalotherwise known as anthracite or a coal consisting for the greater partof glance coal, using preferably coal possessing baking properties;

It has also been found that the-result desired can only be obtained ifthe initial coal is subjected to the treatment withv the solvent in avery pulverulent shape or if the conversion into this pulverulent shapetakes place before the completion of the heat treatment in the presenceof the hydrocarbon oils.

The size of particles must be less than 9.5 mm. As treating agentsaccording to the invention, hydrocarbon oils may be used, chiefly coaltar oils, such as, for instance, anthracene oil.

It is recommended to use these oils in excess,

, product obtained shows the desired since otherwise overheating willhardly be avoided, which would result in disturbing decompositions.Suitably a considerable .surplus of liquid treating agents is used and,e. g., a-ratio in weight of oil to coal of 5 to 1 is used; Part of theoil may be added in the course of the process.'

If a'coking glance coal having a grain size of, say, 0.1 mm. is treatedwith the flveto sixfold amount or anthracene oil at temperatures where adecomposition of the coal cannot take'placee. g., at temperaturespf 360C.-for about 3 or 4 hours and then abQutbne-half-is distilled withoutbeing separated from the undissolved matter at ordinary pressure, abituminous product showing surprisingly good properties willbe obtained.

Theefiect occurring with the process of the invention may be accountedfor by the supposition that the individual particles of coal swell up inthe oil without undergoing decomposition.

The temperature of treatment must be chosen in such a manner as toprevent decomposition oi the coal, but-on the other hand-it must not betoo low, as otherwise the desired bitumen-like state which must beconsidered a colloidal solution of coal in the treating agent will not.be obtained or will be imperfect.

The optimum temperature of treatment for each individual case. can beeasily ascertained by simple preliminary tests. also the time oftreatment which is suitable in the individual case and this variesslightly depending on the temperature used and the initialmateriala Thetime of treatment must be chosen of such length that the final colloidalproperties. 'To exceed the time of treatment involves no risk, since noreversion will take place if care is taken to avoid overheating.

To remove the used surplus of solvent, it is necessary to distill thisexcess solvent after the heat treatment, when care must be taken againthat decompositions are avoided.

The-use of vacuum or other costly means of distillation is notnecessary, as has been found out.

Depending on the desired application of the final product, a more orless great amount 'of solvent may be left, in the final product.However, excessive amountsof the solvent must'not be removed, asotherwise the'colloidal nature and thus the favorable properties mightbe impaired. Those products have proved satisfactory which possess aratio of coal to oil-of, say. 1:2 or 1:3. I

When using vacuum with the distillation one will succeed in removing agreater amount of Marv products obtained in 2 mist withsui impairing theproperties of the final product and without affecting the colloidalnature.

In its behavior the final product resembles'the mineral oil bitiunen,especially the softening point and breaking point are similar to thoseof the bitumen. so that the great interval between thesetwo points maybe considered as useful properties of the final product obtained by theprocess according-to the invention.

In the same manner as bitumen, the product of the present inventionshows a colloidal nature.

Thereby it differs materially from pitch which isof no colloidal natureand, by the way, shows a far smaller interval between the softening andbreaking points.

When using the products forthe insulation ofpipes, this differentbehavior makes itself felt to advantage.

Bitumen used for the manufacture of pipes is required, for instance, topossess a softening point of 90-100 C. according to Kramer-Sarnow and abreaking point below -5 C. according to Fraasz. At least these valueswill be obtained in the prodnot of bitumen made in accordance with theinvention.

v The special pitches made for the purposes of I insulation-of pipeshave never attained the cited Physical values: in particular thesespecial pitches show, after the evaporation test, a break ing pointmostly materially above 0 0., which renders their use impossible, forinstance, in winter time.

As an example the following test report may Filled amount, lal igrams:residue of distillation, 907 grams=50%.

Properties of the same after adding a filler in the form of limestonedust:

Softening point according to Kramer-Sarnow 91 C. Softening point afterevaporation 95 C. Loss on evaporation 2% Breaking point according toFraasz Above 15' C. Breaking point accordingv to Fraasz afterevaporation. Above 15' C.

It has been already mentioned that the products made according to theinvention are partic-' ularly adapted forthe purposes of pipe insulation. If n, fillers may be added to them. Such materials will be used attemperatures not exceedingl80 0., since higher temperatures are likelyto cause deteriorations. At these temperatures below 180' C., sometim vif accordance with the invention are mixed with flllt mobility doesnot-exist. i. e., the material has too high a viscosity, so that thenecessary thickness of insulation of the pipes to be wrapped will beexceeded. Exceeding the thickness of insulation in such a manner willresult in troubles, apart from the fact that unevennesses are likely tooccur and useless extra consumption will be the result.

Now it has been found that the addition of coal tar, particularly hightemperature tar, similar to pitch, may influence the viscosity of thebitumen-like material, even if mixed with appreciable quantities offillers, in such a satisfactory manner that no difllculties will beencountered in the installation at temperatures of 180 C. and less,without the breaking point of the compound being reduced unduly.

With these compounds it is by no means possible to create the desiredlower viscosity. say, by

' addition of any materials, e'. g., solvents, since a productcontaining a high percentage of solvents shows softening points below'7080 C., i. e., the compound becomes so mobile that it may be used forthe insulation of pipes at 180 C. and less, but it becomes useless inother respects. When proceeding in accordance with the invention, viz.,when adding pitch or coal tar, the drawbacks will not be experienced.While a lowering of the breaking point cannot be avoided, the breakingpoints are within therange required for natural bitumens, thus theincreased mobility will not be obtained at the expense of a greatdisadvantage.

According to the invention, pitch is added tq the product of the processdisclosed either before or simultaneously with or after the admixture offillers, or the process may be carried out in such a manner that eithertar or pitch is added in the course of the process for the manufactureof the bitumen-like materials; for instance, a mixture of pulverulentglance coal, coal tar oils and pitch may be subjected to the heattreatment disclosed in the principal patent or the addition may be madeafter the heat treatment and prior to the distillation of the surplussolvent.

In all instances, products showing improved properties will be obtained.

The amount of the admixture may vary within comparatively wide limits;in most cases an addition of pitch ranging from 10 to 20% will besuflicient to make the compound mobile enough at working temperatures offrom to 180 C.

The most suitable addition is hard pitch. Such hard pitch is mixed,preferably in a reduced shape, with a bitumen-like material obtained bythe process disclosed; the admixture of filters may take placesimultaneously with the addi-. tion of the hard pitch. .Naturally, auniform mixing should be striven for.

The curves shownin Figs. 1 and 2 of the drawings reveal the influenceupon the viscosity of a pipe wrapping substance and the ei'iect on thebreaking point when adding different amounts of hard pitch. Theviscosity is expressed by the adhesive quantity per square decimeter atC. It will be noted that the viscosity is influenced to advantagewithout the breaking point being loweredunduly.

I claim:

1. Process for the production of bitumen-like materials, wherein glancecoal or anthracite or coal consisting chiefly of glance coal is treatedin a pulverulent form with coal tar oils, at increased temperaturesrangl l below the decomposition temperatures of the coal, and excesssolvent is distilled from the resulting product of said treatmentwithout elimination of the solid constituents.

2. Bitumen-like product from a mixture of glance coal and a hydrocarbonoil of high boiling point, whereinsaid product in colloidal state showsa softening point of more than 90 C. and a breaking point of less thanC.

3.Process for the production of bitumen-like materials, whereinanthracite coal is ground to a particle size of from one to five-tenthsmillimeter and treated with from four to six times its weight ofanthracene oil at a temperature of from 350 to 370 centigrade, theexcess solvent oil being distilled oif until its remainder is only twoto three times the weight of initial coal in the final product.

4. Process for the production of insulation for pipes, whereinanthracite coal is ground to a particle size of from one to five-tenthsmillimeter, and treated with from four to six times its weight ofanthracene oil at a temperature 01' from 350 to 370 centigrade, theexcess solvent being distilled oil until its remainder is only two tothree times the weight of initial coal in the final product, and fillermaterial is added, wherein 10 to 20% of hard pitch is added prior toaddition of the filler material to reduce the viscosity but not to lowerthe breaking point.

5. Process for the production 01 colloidal, bitumen-like materials,wherein coal consisting chiefly of glance coal and of a grindingfineness of less than half a millimeter, is treated with coal tar oil atincreased temperatures ranging below the decomposition temperatures ofthe coal, and excess coal tar oil is distilled from the resultingproduct of said treatment without elimination of ihe solid constituents.

6. Process for the production of colloidal bitumen-like materials,wherein glance coal is treated in pulverulent form with anthracene oilat increased temperatures ranging below the decomposition temperatureoi. the coal, and excess anthracene oil is distilled from the resultingproduct or said treatment without elimination of the solid constituents.

7. Process for the production of colloidal bitumen-iike materials,wherein anthracite coal of a grinding fineness of half a millimeter istreated with a surplus of from four to six times by weight of coal taroil at increased temperatures ranging below the decompositiontemperature of the coal, and excess coal tar oil is distilled ofl fromthe resulting product of said treatment without elimination of the solidconstituents. v

8. Process for the production of colloidal bitumen-like materials,wherein anthracite coal of a decomposition temperature above 370' C. istreated in pulverulent form with coal tar oil at a temperature from 350C. to 370 C. and excess coal tar oil is distilled oflirom the resultinproduct of said treatment without elimination of the solid constituents.

9. Process for the production of colloidal bitumen-like materials,wherein anthracite coal is treated in pulverulent form with a coal taroil, at increased temperature ranging below the decompositiontemperature of the coal, and excess solvent is distilled off until thesolvent amounts to only'two or three times the amount oi? initial coalin the final product.

10. Colloidal bitumen-like product from a mixture of undecomposedanthracite "coal and a coal tar oil, having a softening point of morethan C. and a breaking point oi less than 0' C.

11. Colloidal bitumen-like product from a mixture of undecomposed glancecoal and anthracene oil, having a softening point of more than 90 C. anda breaking point of less than 0 C.

12. Process for the production of bitumen-like materials, wherein glancecoal or anthracite coal consisting chiefly of glance coal is treated inpulverulent form with a coal tar oil, at increased temperatures rangingbelow the decomposition temperatures of the coal, and excess solvent isdistilled from the resulting product of said treatment withoutelimination of the solid constituents, and filler material is added,wherein 10 to 20% of hard pitch is added prior to the addition of thefiller material to reduce the. viscosity but not to lower the breakingpoint, for the production of insulation for pipes.

' mom JENKNER.

